反应详情

51.1 g of methyltoluphenylphosphonium bromide was added to a mixture of 16.1 g tert-butoxy potassium and 500 ml tetrahydrofuran, and then stirred for 1 hr and 20 min at room temperature. 16.1 g of benzyl 4-oxo-1-piperidinecarboxylate was added thereto, and the mixture was stirred for 2 hr and 40 min at room temperature. The reaction solution was evaporated, diethyl ether was added thereto, and then filtered through Celite. The filtrate was washed with water and brine, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was evaporated, and the resulting residue was subjected to silica gel-column chromatography to give 25.5 g of benzyl 4-methylene-1-piperidinecarboxylate.

1. stirringthe mixture was stirred for 2 hr and 40 min at room temperature
2. customThe reaction solution was evaporated
3. additiondiethyl ether was added
4. filtrationfiltered through Celite
5. washThe filtrate was washed with water and brine
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltered
8. customThe filtrate was evaporated